JP4576999B2 - Method for producing self-flowing hydraulic composition - Google Patents

Description

  The present invention is a method for producing a self-flowing hydraulic composition using a hydraulic component containing Portland cement, which can be used as a self-leveling material having excellent self-fluidity that can be used mainly for floor foundation adjustment of general buildings. About.

As a self-leveling self-flowing hydraulic composition, Patent Document 1 discloses a hydraulic component composed of alumina cement, Portland cement, gypsum, blast furnace slag, a coagulation regulator composed of a lithium salt and a boric acid compound, a water reducing agent, A composition comprising a thickener is disclosed.
Patent Document 2 discloses a composition comprising a hydraulic component composed of alumina cement, Portland cement, gypsum, and blast furnace slag, a water reducing agent, and a thickening agent.

JP 2000-211961 A JP 2000-302519 A

Self-flowing hydraulic composition (SL material) with self-leveling can form a flat surface with excellent surface accuracy just by mixing and pouring with water. In order to save labor and improve work efficiency, it is widely used mainly for building plastering finishing methods.
Self-leveling materials are manufactured by blending hydraulic components such as Portland cement and additives such as water reducing agents and / or thickeners, and must have high fluidity and a smooth surface with high precision. Is a requirement.
However, in the self-leveling material containing Portland cement as a hydraulic component, variation in the fluidity of the resulting slurry is recognized between production lots. For this reason, the product yield may be deteriorated, resulting in problems in productivity and economy.
The present invention is a self-flowing hydraulic composition in which the fluidity of the slurry does not vary between production lots, the fluidity is stable, and the product yield during production is improved in self-leveling materials containing Portland cement as a hydraulic component. The purpose was to propose a manufacturing method of the product.

The present invention provides a self-flowing hydraulic composition comprising a hydraulic component containing Portland cement, a water reducing agent and / or a thickening agent,
Measure the amount of free calcium oxide contained in Portland cement,
Portland cement uses Portland cement with a free calcium oxide content of 1% by mass or less,
A method for producing a self-flowing hydraulic composition, comprising mixing a hydraulic component containing Portland cement having a free calcium oxide content of 1% by mass or less with a water reducing agent and / or a thickening agent.
In the present invention, the amount of free calcium oxide is a value obtained by applying the method described in “Quantitative Method of Free Calcium Oxide Glycerin-Alcohol Method (Method B)” described in Cement Association Standard Test Method JCAS I-01-1997. It is. Therefore, the amount of free calcium oxide of the present invention is a value that includes the quantitative value of calcium hydroxide together with the amount of free calcium oxide.

The preferable aspect of the manufacturing method of the self-flowing hydraulic composition of this invention is shown below. A plurality of preferred embodiments can be combined.
1) The hydraulic component should contain 10% by weight or more of Portland cement in 100% by weight of the hydraulic component.
2) The hydraulic component further contains at least one component selected from alumina cement and gypsum.
3) The hydraulic component is 10 to 100% by mass of Portland cement (excluding 100% by mass), 0 to 90% by mass of alumina cement and 0 to 90% by mass of gypsum (however, the total of Portland cement, alumina cement and gypsum) Is 100 mass%).
4) The self-flowing hydraulic composition further contains an inorganic component,
An inorganic component contains 10-350 mass parts with respect to 100 mass parts of hydraulic components.
5) The self-flowing hydraulic composition further contains fine aggregate, and the fine aggregate contains 50 to 500 parts by mass with respect to 100 parts by mass of the hydraulic component.
6) The self-flowing hydraulic composition further contains a setting modifier.
7) It contains 0.01-1.0 mass part of water reducing agents and / or 0.05-1.0 mass part of thickeners with respect to 100 mass parts of hydraulic components.
8) The self-leveling SL value (L30 / L0) is 0.90 or more.

  The present invention adds a step of measuring the amount of free calcium oxide of Portland cement in producing a self-flowing hydraulic composition, and as Portland cement, the amount of free calcium oxide contained in Portland cement is 1% by mass or less. By using the product, a product with stable fluidity of the self-leveling material slurry can be obtained, the quality between production lots is stabilized, the yield in production is improved, and as a result, productivity, economy and quality are excellent. It is a manufacturing method of a self-flowing hydraulic composition.

The method for producing a self-flowing hydraulic composition of the present invention is a method for producing a self-flowing hydraulic composition comprising a hydraulic component containing Portland cement, a water reducing agent and / or a thickening agent.
Measure the amount of free calcium oxide contained in Portland cement,
Portland cement having a free calcium oxide content of 1% by mass or less, preferably 0.95% by mass or less, more preferably 0.9% by mass or less, more preferably 0.85% by mass or less, and particularly preferably 0.82% by mass or less. A self-flowing hydraulic composition can be produced by blending or mixing with a hydraulic component containing a water reducing agent and / or a thickening agent.
The method for producing a self-flowing hydraulic composition of the present invention comprises a step of measuring the amount of free calcium oxide contained in Portland cement, and a measured value of the amount of free calcium oxide contained in Portland cement as a hydraulic component is 1 mass. % Or less, preferably 0.95% by weight or less, more preferably 0.9% by weight or less, more preferably 0.85% by weight or less, particularly preferably 0.82% by weight or less of Portland cement. It is a method for producing a self-flowing hydraulic composition characterized by using a hydraulic component containing Portland cement, a water reducing agent and / or a thickening agent, and having a stable fluidity as a self-leveling material. As a result, the quality of the fluidity of the product (slurry) is stabilized between production lots, and productivity and economy are improved.

  The method for measuring the amount of free calcium oxide contained in Portland cement is the “quantification method of free calcium oxide, ethylene glycol method (method A)” described in the Standard Test Method JCAS I-01-1997 of Cement Association, A known method such as “quantification method glycerin-alcohol method (Method B)” can be used. In the present invention, the amount of free calcium oxide (f-CaO amount) is the standard test method JCAS I-01-1997 of the Cement Association. It is the value calculated | required by applying the method as described in "The determination method of a free calcium oxide glycerol-alcohol method (B method)". Therefore, the amount of free calcium oxide (f-CaO amount) of the present invention is a value that includes the quantitative value of calcium hydroxide as well as the amount of free calcium oxide.

  In the method for producing a self-flowing hydraulic composition of the present invention, a lot in which the measured value of free calcium oxide contained in Portland cement exceeds 1% by mass is homogeneously mixed with other lots and contained in Portland cement. When the amount of free calcium oxide to be measured is measured and the measured value of the amount of free calcium oxide contained in Portland cement is 1% by mass or less, it can be used.

A self-flowing hydraulic composition containing a hydraulic component containing Portland cement and a water reducing agent and / or a thickening agent,
1) The self-flowing hydraulic composition is a composition containing a hydraulic component containing Portland cement and a water reducing agent.
2) Self-fluidic hydraulic composition In the case of a composition comprising a Portland cement and a thickener, or 3) Self-fluidic hydraulic composition A hydraulic component containing Portland cement and a water reducing agent And in the case of a composition containing a thickener.

The hydraulic component is preferably 10 to 100% by mass of Portland cement (excluding 100% by mass), 0 to 90% by mass of alumina cement and 0 to 90% by mass of gypsum (however, the total of Portland cement, alumina cement and gypsum) Is 100% by mass), more preferably 10 to 100% by mass of Portland cement (excluding 100% by mass), 0 to 80% by mass of alumina cement, and 0 to 70% by mass of gypsum,
More preferably, Portland cement 15 to 100% by mass (except 100% by mass), alumina cement 0 to 70% by mass and gypsum 0 to 60% by mass,
Particularly preferably, Portland cement is 20 to 100% by mass (excluding 100% by mass), alumina cement is 0 to 60% by mass, and gypsum is 0 to 50% by mass (however, the total of Portland cement, alumina cement and gypsum is 100% by mass) Can be used.

  As the Portland cement, ordinary Portland cement, early-strength Portland cement, or the like can be used. Use of Portland cement as the hydraulic component is preferable because it is effective for cost reduction.

  As for the gypsum, each gypsum such as anhydrous or semi-water can be used as one kind or a mixture of two or more kinds regardless of the kind. Gypsum is rapidly hardened and acts as a component for maintaining dimensional stability after curing.

Alumina cement has a potentially rapid hardening property, and gives a cured product excellent in chemical resistance and fire resistance after curing. In addition, due to the presence of blast furnace slag having latent hydraulic properties, a decrease over time in the strength of the cured body, which is a drawback thereof, is also suppressed. Alumina cement is commercially available is known several those mineral composition is different, but both major component is monocalcium aluminate (CA), from the viewpoint of strength and coloring, CA component number and C ₄ Alumina cement with a small amount of small components such as AF is preferred.

The self-flowing hydraulic composition can further contain an inorganic component such as blast furnace slag, fly ash, and silica. In particular, by including blast furnace slag, the crack resistance of the cured product due to drying shrinkage can be enhanced.
The addition amount of the inorganic component is 10 to 350 parts by mass, preferably 30 to 200 parts by mass with respect to 100 parts by mass of the hydraulic component.

The amount of blast furnace slag added is preferably 10 to 350 parts by mass with respect to 100 parts by mass of the hydraulic component. If the amount is too small, the shrinkage increases, and if too much, the strength may be reduced.
As the blast furnace slag, a blast furnace slag having a brain specific surface area of 3000 cm ² / g or more as defined in JIS A-6206 can be used.
As the self-flowing hydraulic composition, a mixed cement containing Portland cement and blast furnace slag can be used. The filler used in the mixed cement is blast furnace slag, fly ash, or siliceous mixed material.

The self-flowing hydraulic composition can further include fine aggregate.
The fine aggregate is preferably in the range of 50 to 500 parts by mass, preferably 100 to 400 parts by mass, particularly preferably 150 to 300 parts by mass with respect to 100 parts by mass of the hydraulic component.
As the fine aggregate, an aggregate having a particle size of 2 mm or less, preferably an aggregate having a particle size of 0.1 to 2 mm, more preferably an aggregate having a particle size of 0.2 to 2 mm, particularly preferably 0.3 to 2 mm. Aggregate is the main component.
As fine aggregates, silica sand, river sand, sea sand, alumina clinker, silica powder, clay mineral, waste FCC catalyst, inorganic materials such as limestone, pulverized resin such as urethane crushed, EVA foam, foamed resin, etc. it can.
In particular, as fine aggregates, silica sand, river sand, sea sand, quartz powder, alumina clinker and the like can be preferably used.
The particle size of the fine aggregate is measured using several sieves having different nominal dimensions as defined in JIS Z-8801.

  The self-flowing hydraulic composition can contain a thickener, a water reducing agent, an antifoaming agent, a setting modifier such as a setting accelerator and a setting retarder, and the like.

As the thickener, cellulose-based, protein-based, latex-based, water-soluble polymer-based, and the like can be used, and in particular, cellulose-based can be used.
The addition amount of the thickener can be added within a range that does not impair the characteristics of the present invention, and is 0.05 to 1.0 part by mass, and further 0.1 to 0.7 part with respect to 100 parts by mass of the hydraulic component. It is preferable to include 0.2 parts by mass, particularly 0.2 to 0.5 parts by mass. If the amount of the thickener added is increased, the fluidity may be lowered, which is not preferable.
It is preferable to use a thickener and an antifoaming agent in combination in order to give a favorable effect on the suppression of aggregate separation, the suppression of bubble generation, and the improvement of the surface of the cured body, and to improve the properties as a self-leveling material.

As the antifoaming agent, a known substance such as a synthetic substance such as silicon-based, alcohol-based, or polyether, or a plant-derived natural substance mineral oil can be used.
The addition amount of the antifoaming agent can be added within a range that does not impair the characteristics of the present invention. The following is preferred. When the defoaming agent is added in a larger amount than the above, the defoaming effect may not be improved.

  As the setting modifier, a setting accelerator that is a component that accelerates setting, a setting retarder that is a component that delays setting, and the like can be used alone or in combination.

A known setting accelerator can be used as the setting accelerator. Examples of setting accelerators include inorganic and organic lithium salts such as lithium carbonate, lithium chloride, lithium sulfate, lithium nitrate, lithium hydroxide, lithium acetate, lithium tartrate, lithium malate, lithium citrate, and other organic acids. Lithium salt such as can be used. In particular, lithium carbonate is preferable from the viewpoints of effects, availability, and cost.
As the setting accelerator, it is preferable to use a particle size that does not interfere with the properties, and the particle size is preferably 50 μm or less.
Particularly when a lithium salt is used, the particle diameter of the lithium salt is preferably 50 μm or less, more preferably 30 μm or less, and particularly preferably 10 μm or less. If the particle diameter is larger than the above range, the solubility of the lithium salt is decreased. Then, it may be conspicuous as a large number of fine spots, and the appearance may be impaired.

  As the setting retarder, a known setting retarder can be used. As an example of a set retarder, sodium salts such as inorganic sodium salts and organic sodium salts such as sodium sulfate, sodium bicarbonate, sodium tartrate, sodium malate, sodium citrate, and sodium gluconate can be used. . In particular, sodium bicarbonate and sodium tartrate are preferable from the viewpoints of effect, availability, and price.

Depending on the self-flowing hydraulic component and hydraulic component composition used, the setting modifier can be added as appropriate within the range that does not impair the properties, and the components, addition amount and mixing ratio of the setting accelerator and setting retarder can be adjusted. By appropriately selecting and adding to the self-flowing hydraulic component, the pot life of the self-flowing hydraulic composition can be adjusted, and the use as a self-leveling material becomes very easy, which is preferable.
When the self-fluidic hydraulic composition is used as a self-leveling material, the setting modifier has a total amount of lithium salt and sodium salt of 0.05 to 5 parts by mass with respect to 100 parts by mass of the hydraulic component. It is preferable to add in the range of 1 to 2 parts by mass, particularly 0.3 to 1.00 parts by mass.

As a method for producing a self-flowing hydraulic composition,
The Eirich mixer contains hydraulic components, water reducing agents and / or thickeners and, if necessary, fine aggregates, pozzolanic components, antifoaming agents, setting modifiers such as setting accelerators and setting retarders. A method of mixing and stirring using a stirrer or a mixer.

The self-flowing hydraulic composition obtained by the present invention is mixed with a predetermined amount of water, and the flow value is preferably adjusted to 190 mm or more, more preferably 200 mm or more, particularly preferably 210 mm or more, It is preferable for the reason that it is easy to construct and it is easy to obtain a cured body surface with high smoothness.
The SL value L0 is preferably 400 mm or more, more preferably 420 mm or more, more preferably 440 mm or more, and particularly preferably 500 mm or more. The SL value L30 / L0 (the SL value L30 is set to the SL value L0). The value obtained by dividing by the value of is preferably 0.90 or more, more preferably 0.91 or more, more preferably 0.92 or more, and particularly preferably 0.93 or more. It is preferable for the reason that it is easy to obtain a cured body surface having high thickness and smoothness.
In particular, the SL value L0 is preferably 400 mm or more, more preferably 420 mm or more, more preferably 440 mm or more, particularly preferably 500 mm or more,
SL value L30 is preferably 380 mm or more, more preferably 400 mm or more, particularly preferably 410 mm or more,
SL value L30 / L0 (SL value L30 value divided by SL value L0 value) is preferably 0.90 or more, more preferably 0.91 or more, more preferably 0.92 or more Particularly preferably, it is preferably adjusted to 0.93 or more for the reason that it is easy to obtain a hardened product surface with high ease of construction and high smoothness.

  When the self-flowing hydraulic composition obtained according to the present invention is used as a self-leveling material for adjusting the floor base, water is 95 to 120 parts by mass, more preferably 95 to 115 parts by mass, particularly 100 parts by mass of the hydraulic component. It is preferable to add 100 to 110 parts by mass.

  The self-flowing hydraulic composition obtained by the present invention has a watering time of a slurry produced by mixing with water at 20 ° C. of preferably 60 to 150 minutes, more preferably 65 to 150 minutes, particularly preferably 100. It is preferable to use in the range of ~ 150 minutes.

  The self-flowing hydraulic composition obtained by the present invention can be applied as a self-leveling material by a known method. For example, it is disclosed by Unexamined-Japanese-Patent No. 2001-040862 etc. as an example of construction.

The self-flowing hydraulic composition obtained by the present invention can be used as a self-leveling material mainly used for adjusting the floor foundation of general buildings.
The self-flowing hydraulic composition obtained by the present invention can be widely used as a surface finishing material for concrete, and is a general construction plastering material, for example, synthetic resin such as P-tile sticking, long sheet, carpet, urethane, etc. It can also be used for the construction of the foundation of a painted floor.
The self-flowing hydraulic composition obtained by the present invention has excellent characteristics in a wide temperature range of 40 ° C. or less, preferably 35 ° C. or less, particularly preferably 33 ° C. or less, and can be used as a self-leveling material.

  Hereinafter, the present invention will be described in more detail based on examples. However, the present invention is not limited by the following examples.

(1) Evaluation method of Blaine specific surface area: Measured by using a Blaine air permeation device specified in JIS R-5201.
(2) Measuring method of free calcium oxide content (f-CaO content) contained in Portland cement: “Quantitative method of free calcium oxide glycerin-alcohol method (described in JCAS / I-01-1997) Measurement is carried out by applying the method described in "Method B)".

(3) Evaluation of slurry: Evaluation is performed at a temperature of 20 ° C. or 30 ° C. shown in Tables 2 to 4.
-Flow value: Measured according to JASS 15M-103. After filling a concrete composition in which a vinyl chloride pipe (internal volume: 100 ml) having an inner diameter of 50 mm and a height of 51 mm is placed on a glass sheet having a thickness of 5 mm and kneaded, the pipe is pulled up. After the spread has stopped, the diameters in two perpendicular directions are measured, and the average value is taken as the flow value.
Self-leveling: Using a SL measuring device shown in FIG. 1, a rail is provided on a rail 30 mm wide x 30 mm high x 750 mm long, 150 mm long from the tip, and a predetermined amount of slurry immediately after kneading is provided. Fill and mold. Immediately after molding, the weir plate is pulled up, and after the flow of the slurry is stopped, the distance from the gauge point (the installation portion of the weir plate) to the shortest portion of the slurry flow is measured, and the value (SL value) is defined as L0.
Similarly, 30 minutes after molding, the weir plate is pulled up, and after the flow of the slurry is stopped, the distance from the gauge point (the installation portion of the weir plate) to the shortest portion of the slurry flow is measured, and the value (SL value) is L30. And

(4) Surface condition (water floating, aggregate separation, presence or absence of white flower, unevenness, bubble trace):
In the separation of the aggregate, in the self-leveling property of (3), it is observed by palpation whether the aggregate is stopped in the middle of the slurry after the flow of the slurry is stopped.
As for water floating, whether or not the breathing water after pulling up the weir plate flows faster than the slurry itself, and only the water does not flow for a long time, the presence or absence of white flower, irregularities, and bubble traces are obtained in (2) above. The slurry was poured into a 30 cm × 30 cm concrete plate at a thickness of 10 mm, and visually observed after the curing was completed. Evaluation was as follows.
○: None, ×: Present

(5) Watering time (minutes):
The slurry obtained in the above (2) was poured into a 30 cm × 30 cm concrete plate at a thickness of 10 mm, and the time when water on the slurry surface disappeared (watering) was visually observed and evaluated.

(6) Materials used: The following materials were used.
Alumina cement: Blaine specific surface area 3,600 cm ² / g, monocalcium aluminate content 45% by mass.
Portland cement: early strong cement, Blaine specific surface area 4,500 cm ² / g.
Gypsum: type II anhydrous gypsum, Blaine specific surface area 3,300 cm ² / g.
Blast furnace slag: Blaine specific surface area 4,400 cm ² / g.
Silica sand: No. 4 silica sand (commercial product).
Lithium salt: Lithium carbonate (commercially available).
Aluminum salt: Aluminum sulfate salt (commercially available).
Sodium salt: sodium bicarbonate, sodium tartrate, sodium gluconate (all are commercially available products).
-Water reducing agent: Polycarboxylic acid water reducing agent (commercially available).
-Thickener: Methylcellulose thickener (commercially available).
-Antifoaming agent: Polyether type antifoaming agent (commercially available product).

(Comparative Examples A and B, Example 3-5, Comparative Example 1-4) Preparation of the hydraulic composition and slurry, Rating:
The hydraulic components, blast furnace slag, fine aggregate, water reducing agent, thickener, setting modifier, antifoaming agent (total amount: 1.5 kg) shown in Table 1 (SL-1) are kneaded using a chemistor, The hydraulic composition was prepared, and a predetermined amount of water was further added and kneaded for 3 minutes to obtain a slurry (SL-1). The hydraulic composition and the slurry were adjusted at 20 ° C. As the Portland cement to be used, the amount of f-CaO contained in Portland cement was measured in advance, and those shown in Table 2 were used.

( Comparative Example C, Example 7 , Comparative Examples 5 and 6) Preparation and evaluation of hydraulic composition and slurry:
The hydraulic components, blast furnace slag, fine aggregate, water reducing agent, thickener, setting modifier, antifoaming agent (total amount: 1.5 kg) shown in Table 1 (SL-2) are kneaded using a chemistor, The hydraulic composition was adjusted, and a predetermined amount of water was added and kneaded for 3 minutes to obtain a slurry (SL-2). The hydraulic composition and the slurry were adjusted at 30 ° C. As the Portland cement to be used, the amount of f-CaO contained in Portland cement was measured in advance, and those shown in Table 3 were used.

( Reference Example 8, Comparative Example 7) Preparation and evaluation of hydraulic composition and slurry:
The hydraulic components, blast furnace slag, fine aggregate, water reducing agent, thickener, setting modifier, antifoaming agent (total amount: 1.5 kg) shown in Table 1 (SL-3) are kneaded using a chemistor, The hydraulic composition was prepared, and a predetermined amount of water was further added and kneaded for 3 minutes to obtain a slurry (SL-3). The hydraulic composition and the slurry were adjusted at 20 ° C. As the Portland cement to be used, the amount of f-CaO contained in Portland cement was measured in advance, and those shown in Table 4 were used.

It is a figure which shows schematically self-leveling property evaluation using SL measuring device.

Claims (8)

In a method for producing a self-flowing hydraulic composition comprising a hydraulic component comprising Portland cement and alumina cement, and a water reducing agent and / or a thickening agent,
Measure the amount of free calcium oxide contained in Portland cement,
Portland cement uses Portland cement having a free calcium oxide content of 0.67 to 0.79% by mass,
A hydraulic component containing Portland cement having a free calcium oxide amount of 0.67 to 0.79% by mass, and a water reducing agent and / or a thickener are mixed ,
The hydraulic component contains 10% by mass or more of Portland cement in 100% by mass of the hydraulic component, and a method for producing a self-flowing hydraulic composition.   The method for producing a self-flowing hydraulic composition according to claim 1, wherein the hydraulic component further contains gypsum. The hydraulic component is 10 to 100% by mass of Portland cement (excluding 100% by mass), 0 to 90% by mass of alumina cement and 0 to 90% by mass of gypsum (however, the total of Portland cement, alumina cement and gypsum is 100% by weight.) the method for manufacturing the self-flowability hydraulic composition according to claim 1 or 2, characterized in that it comprises a. The self-flowing hydraulic composition further includes at least one inorganic component selected from the group consisting of blast furnace slag, fly ash and silica,
The method for producing a self-flowing hydraulic composition according to any one of claims 1 to 3 , wherein the inorganic component contains 10 to 350 parts by mass with respect to 100 parts by mass of the hydraulic component. The self-flowing hydraulic composition further comprises fine aggregate,
The method for producing a self-flowing hydraulic composition according to any one of claims 1 to 4 , wherein the fine aggregate contains 50 to 500 parts by mass with respect to 100 parts by mass of the hydraulic component. The method for producing a self-fluidic hydraulic composition according to any one of claims 1 to 5 , wherein the self-fluidic hydraulic composition further contains a setting modifier. Per 100 parts by mass of hydraulic component, it claims 1-6, characterized in that it comprises a water reducing agent 0.01-1.0 parts by weight and / or thickening agent 0.05 to 1.0 parts by weight A process for producing a self-fluid hydraulic composition as described in Item 1. The self-fluidic hydraulic composition production method according to any one of claims 1 to 7 , wherein the self-leveling SL value (L30 / L0) is 0.90 or more.

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